Lithium Hydroxide → HCID 10473396, compound

HRID 418465Notes

Reaction equation

HRID 418465 reaction equation
[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][C:13]([O:15]C)=[O:14])[C:7]([CH3:17])=[C:6]2[C:18]1[C:27]2[C:22](=[C:23]([CH3:28])[CH:24]=[CH:25][CH:26]=2)[N:21]=[CH:20][CH:19]=1)#[N:2].[OH-].[Li+]>C1COCC1.O>[C:1]([C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([CH2:12][C:13]([OH:15])=[O:14])[C:7]([CH3:17])=[C:6]2[C:18]1[C:27]2[C:22](=[C:23]([CH3:28])[CH:24]=[CH:25][CH:26]=2)[N:21]=[CH:20][CH:19]=1)#[N:2]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 66651938HCID 66651938, compound

Product 1

HCID 10473396HCID 10473396, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

The product from step b) was taken up in THF (10 ml) treated with a solution of lithium hydroxide (252 mg) in water (10 ml) and stirred for 1 hour. The solution was concentrated to remove the THF and acidified with saturated aqueous potassium hydrogen sulphate. The solid was collected by filtration, washed with water, washed with a little cold propan-2-ol, washed with a little cold ether and dried to give the title compound as a yellow/orange solid (606 mg).

Workup

  1. concentrationThe solution was concentrated
  2. customto remove the THF
  3. filtrationThe solid was collected by filtration
  4. washwashed with water
  5. washwashed with a little cold propan-2-ol
  6. washwashed with a little cold ether
  7. customdried

Sources & evidence

ORD record
ord-e267ac59ebff41e7995d93e13554cb73
Source dataset
uspto-grants-2012_01
Patent number
US08093278B2

Reaction notes

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